US11560320B2 - Solid electrolyte material and battery - Google Patents

Solid electrolyte material and battery Download PDF

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US11560320B2
US11560320B2 US16/915,424 US202016915424A US11560320B2 US 11560320 B2 US11560320 B2 US 11560320B2 US 202016915424 A US202016915424 A US 202016915424A US 11560320 B2 US11560320 B2 US 11560320B2
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solid electrolyte
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Tetsuya Asano
Akihiro Sakai
Masashi Sakaida
Yusuke Nishio
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Panasonic Intellectual Property Management Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00—Compounds of zirconium
    • C01G25/006—Compounds containing, besides zirconium, two or more other elements, with the exception of oxygen or hydrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00—Compounds of rare earth metals
    • C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
    • C01F17/36—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 halogen being the only anion, e.g. NaYF4
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G29/00—Compounds of bismuth
    • C01G29/006—Compounds containing, besides bismuth, two or more other elements, with the exception of oxygen or hydrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G33/00—Compounds of niobium
    • C01G33/006—Compounds containing, besides niobium, two or more other elements, with the exception of oxygen or hydrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G35/00—Compounds of tantalum
    • C01G35/006—Compounds containing, besides tantalum, two or more other elements, with the exception of oxygen or hydrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/006—Compounds containing, besides zinc, two ore more other elements, with the exception of oxygen or hydrogen
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
    • H01M10/0562—Solid materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/74—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by peak-intensities or a ratio thereof only
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0065—Solid electrolytes
    • H01M2300/0068—Solid electrolytes inorganic
    • H01M2300/008—Halides
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • Japanese Unexamined Patent Application Publication No. 2011-129312 discloses an all-solid battery using a sulfide solid electrolyte.
  • FIG. 1 is a sectional view illustrating the schematic configuration of a battery according to Embodiment 3;
  • FIG. 2 is a schematic view illustrating a method of evaluating ion conductivity
  • FIG. 3 is a graph illustrating evaluation results of ion conductivity provided by AC impedance measurement
  • FIG. 4 B is a graph illustrating XRD patterns in Examples A1-A11;
  • FIG. 6 A is a graph illustrating XRD patterns in Examples B1-B13;
  • FIG. 6 B is a graph illustrating XRD patterns in Examples B1-B13;
  • FIG. 8 is a graph of relationships between lithium-ion conductivity and a ave /a LiX in Examples A1-A11 and B1-13 and Comparative Examples 1-3.
  • a plurality of atoms of X form a sublattice having a closest packed structure.
  • solid electrolyte material according to Embodiment 1 having the above-described features provides an all-solid secondary battery having good charge/discharge characteristics.
  • the solid electrolyte material according to Embodiment 1 provides a sulfur-free all-solid secondary battery.
  • the solid electrolyte material according to Embodiment 1 does not have a composition that generates hydrogen sulfide upon exposure to the air (for example, the composition of Japanese Unexamined Patent Application Publication No. 2011-129312). This provides an all-solid secondary battery that does not generate hydrogen sulfide and has high safety.
  • the X-ray diffraction pattern is converted such that the abscissa axis represents, instead of diffraction angle 2 ⁇ , q/q 2 , to provide a second conversion pattern including a peak in at least one selected from the group consisting of a first range of q/q 2 of 0.50 or more and 0.52 or less, a second range of q/q 2 of 1.28 or more and 1.30 or less, and a third range of q/q 2 of 1.51 or more and 1.54 or less.
  • q 2 is a value of q corresponding to the reference peak in the first conversion pattern.
  • the solid electrolyte material according to Embodiment 1 may satisfy: a ave /a LiX >1.018 (1)
  • q 2 is the above-described value of q 2 .
  • q 4 is a value of q at the peak included in the third range.
  • the solid electrolyte material according to Embodiment 1 may include a first crystal phase.
  • the first crystal phase may be a crystal phase that provides the above-described characteristic diffraction pattern.
  • the inventors performed studies and, as a result, have found that, when anions have a hexagonal closest packed structure and satisfy Formula (1) above, a high lithium-ion conductivity of 1 ⁇ 10 ⁇ 4 S/cm or more is provided. This is inferentially achieved because the expanded lattices promote conduction from octahedral sites to metastable tetrahedral sites, which is the rate-determining step of ion conduction.
  • This feature provides a solid electrolyte material having a higher lithium-ion conductivity.
  • the first crystal phase that provides the above-described characteristic diffraction pattern is not limited to a specific crystal structure, and may be, for example, the following crystal structure.
  • the solid electrolyte material according to Embodiment 1 may include a different crystal phase having a crystal structure different from that of the first crystal phase.
  • the weighted average of the proximate peaks may be calculated in terms of the peak positions and the peak intensities to determine q 1 to q 4 .
  • q 1 (q 11 I 11 +q 12 I 12 )/(I 11 +I 12 ).
  • the number of moles of cations may be smaller than the number of moles of anions. In this case, vacant sites for conduction of lithium ions are formed to increase the ion conductivity.
  • Embodiment 2 will be described. Some descriptions having been described in Embodiment 1 above may not be repeated.
  • a solid electrolyte material according to Embodiment 2 has, in addition to the above-described features of the solid electrolyte material according to Embodiment 1, the following features.
  • the X-ray diffraction pattern of the solid electrolyte material according to Embodiment 2 is converted such that the abscissa axis represents, instead of diffraction angle 2 ⁇ , q, to provide a first conversion pattern including a reference peak in a range of q of 1.76 ⁇ ⁇ 1 or more and 2.18 ⁇ ⁇ 1 or less.
  • the X-ray diffraction pattern is converted such that the abscissa axis represents, instead of diffraction angle 2 ⁇ , q/q 1 ′, to provide a second conversion pattern including a peak in at least one selected from the group consisting of a first range of q/q 1 ′ of 1.14 or more and 1.17 or less, a second range of q/q 1 ′ of 1.62 or more and 1.65 or less, a third range of q/q 1 ′ of 1.88 or more and 1.94 or less, and a fourth range of q/q 1 ′ of 1.9 or more and 2.1 or less.
  • q 1 ′ is a value of q corresponding to the reference peak in the first conversion pattern.
  • solid electrolyte material according to Embodiment 2 having the above-described features provides an all-solid secondary battery having good charge/discharge characteristics.
  • the solid electrolyte material according to Embodiment 2 may satisfy: a ave /a LiX >1.018 (1)
  • This feature provides a solid electrolyte material having a high lithium-ion conductivity.
  • q 1 ′ is the above-described value of q 1 ′.
  • q 2 ′ is a value of q at the peak included in the first range.
  • q 3 ′ is a value of q at the peak included in the second range.
  • q 4 ′ is a value of q at the peak included in the third range.
  • q 5 ′ is a value of q at the peak included in the fourth range.
  • c i ′ 0.
  • a LiX is Formula (3) described above in Embodiment 1.
  • the solid electrolyte material according to Embodiment 2 may include a second crystal phase.
  • the second crystal phase may be a crystal phase that provides the above-described characteristic diffraction pattern.
  • the solid electrolyte material according to Embodiment 2 may include the second crystal phase.
  • anions form a sublattice having a structure in which atoms are arranged in a cubic closest packed structure or a distorted cubic closest packed structure; and, in the structure, compared with crystals having a rock-salt structure and composed of Li and a halogen, the lattice constant corresponding to the rock-salt structure is 1.8% or more expanded.
  • the lattice constant corresponding to the rock-salt structure is 1.8% or more expanded.
  • the inventors performed studies and, as a result, have found that, when anions have a cubic closest packed structure and satisfy Formula (1) above, a high lithium-ion conductivity of 1 ⁇ 10 ⁇ 4 S/cm or more is provided. This is inferentially achieved because the expanded lattices promote conduction from octahedral sites to metastable tetrahedral sites, which is the rate-determining step of ion conduction.
  • the second crystal phase that provides the above-described characteristic diffraction pattern is not limited to a specific crystal structure, and may be, for example, the following crystal structure.
  • Li 3 ErBr 6 (hereafter, also referred to as LEB) structure having a crystal structure belonging to the space group C2/m.
  • LEB Li 3 ErBr 6
  • the detailed atomic arrangement of the structure is illustrated in Inorganic Crystal Structure Database (ICSD) (ICSD No. 50182).
  • Other examples include a spinel structure and an inverse spinel structure belonging to the space group Fd-3m and Imma, for example.
  • the solid electrolyte material according to Embodiment 2 may include a different crystal phase having a crystal structure different from that of the second crystal phase.
  • This feature provides a solid electrolyte material having a higher lithium-ion conductivity.
  • the weighted average of the proximate peaks may be calculated in terms of the peak positions and the peak intensities to determine q 1 ′ to q 5 ′.
  • the weighted average of peaks that are equivalent in consideration of imaginary higher order symmetry may be calculated.
  • the above-described LYB structure which is a monoclinic crystal structure, can be regarded as, with focus on the arrangement of anions alone, a distorted cubic closest packed structure as described above.
  • the (20-2) plane and the (131) plane of the LYB structure are approximately equivalent to the (200) plane of the rock-salt structure.
  • weighted average calculated using weights of intensities of both peaks may be used to determine q x ′.
  • the number of moles of cations may be smaller than the number of moles of anions. In this case, vacant sites for conduction of lithium ions are formed, which results in an increase in the ion conductivity.
  • the shape of the solid electrolyte material according to Embodiment 1 or 2 is not particularly limited, and may be, for example, an acicular shape, a spherical shape, or an elliptical spherical shape.
  • the solid electrolyte material according to Embodiment 1 or 2 may be particles. A plurality of particles may be stacked and then pressed so as to have a pellet shape or a plate shape.
  • the solid electrolyte material according to Embodiment 1 or 2 when it has a particulate shape (for example, a spherical shape), it may have a median diameter of 0.1 ⁇ m or more and 100 ⁇ m or less.
  • the median diameter may be 0.5 ⁇ m or more and 10 ⁇ m or less.
  • the solid electrolyte material may have a smaller median diameter than the active material.
  • This feature provides formation of a better diffusion state of the solid electrolyte material according to Embodiment 1 or 2 and, for example, the active material.
  • range of predetermined value A of value B to value C means “range of B ⁇ A ⁇ C”.
  • the solid electrolyte material according to Embodiment 1 or 2 may be produced by, for example, the following method.
  • Binary-halide raw material powders are prepared so as to provide target constituent elements.
  • a solid electrolyte material having a composition of Li 2.5 Y 0.5 Zr 0.5 Cl 6 LiCl, YCl 3 , and ZrCl 4 are prepared in a molar ratio of 2.5:0.5.05.
  • the species of the raw material powders can be selected to thereby determine the composition of the anions.
  • the raw material powders are sufficiently mixed, and then a mechanochemical milling process is performed to mix, pulverize, and react the raw material powders.
  • firing may be performed in a vacuum or an inert atmosphere.
  • the raw material powders may be sufficiently mixed, and then fired in a vacuum or an inert atmosphere. The firing may be performed under firing conditions of, for example, a range of 100° C. to 650° C. for 1 hour or more.
  • the configuration of the crystal phase, the crystal structure, and the positions of the peaks in the X-ray diffraction pattern obtained using Cu-K ⁇ as the ray source and conversion patterns can be determined by adjusting the raw material ratio and by adjusting the reaction process and reaction conditions of the raw material powders.
  • Embodiment 3 will be described. Some descriptions having been described in Embodiment 1 or 2 above may not be repeated.
  • a battery according to Embodiment 3 is provided using the above-described solid electrolyte material according to Embodiment 1 or 2.
  • the battery according to Embodiment 3 includes a solid electrolyte material, a positive electrode, a negative electrode, and an electrolyte layer.
  • the electrolyte layer is a layer disposed between the positive electrode and the negative electrode.
  • At least one of the positive electrode, the electrolyte layer, and the negative electrode includes the solid electrolyte material according to Embodiment 1 or 2.
  • FIG. 1 is a sectional view illustrating the schematic configuration of a battery 1000 according to Embodiment 3.
  • the battery 1000 according to Embodiment 3 includes a positive electrode 201 , a negative electrode 203 , and an electrolyte layer 202 .
  • the positive electrode 201 includes positive electrode active material particles 204 and solid electrolyte particles 100 .
  • the electrolyte layer 202 is disposed between the positive electrode 201 and the negative electrode 203 .
  • the electrolyte layer 202 includes an electrolyte material (such as a solid electrolyte material).
  • the negative electrode 203 includes negative electrode active material particles 205 and solid electrolyte particles 100 .
  • the solid electrolyte particles 100 are particles composed of the solid electrolyte material according to Embodiment 1 or 2, or particles including, as a main component, the solid electrolyte material according to Embodiment 1 or 2.
  • the positive electrode 201 includes a material having a property of storing and releasing metal ions (such as lithium ions).
  • the positive electrode 201 includes, for example, a positive electrode active material (such as positive electrode active material particles 204 ).
  • the positive electrode active material examples include lithium-containing transition metal oxides (such as Li(NiCoAl)O 2 and LiCoO 2 ), transition metal fluorides, polyanions and fluorinated polyanion materials, transition metal sulfides, transition metal oxyfluorides, transition metal oxysulfides, and transition metal oxynitrides.
  • lithium-containing transition metal oxides such as Li(NiCoAl)O 2 and LiCoO 2
  • transition metal fluorides such as Li(NiCoAl)O 2 and LiCoO 2
  • transition metal fluorides such as Li(NiCoAl)O 2 and LiCoO 2
  • polyanions and fluorinated polyanion materials transition metal sulfides, transition metal oxyfluorides, transition metal oxysulfides, and transition metal oxynitrides.
  • the positive electrode active material particles 204 may have a median diameter of 0.1 ⁇ m or more and 100 ⁇ m or less. When the positive electrode active material particles 204 have a median diameter of less than 0.1 ⁇ m, in the positive electrode, the positive electrode active material particles 204 and the halide solid electrolyte material may not form a good diffusion state. This results in degradation of the charge/discharge characteristics of the battery. When the positive electrode active material particles 204 have a median diameter of more than 100 ⁇ m, lithium diffuses slowly in the positive electrode active material particles 204 . This may make it difficult for the battery to operate at a high power.
  • the positive electrode active material particles 204 may have a median diameter larger than the median diameter of the halide solid electrolyte material. This results in a good diffusion state of the positive electrode active material particles 204 and the halide solid electrolyte material.
  • the volume ratio “v:100 ⁇ v” of the positive electrode active material particles 204 and the halide solid electrolyte material included in the positive electrode 201 may satisfy 30 ⁇ v ⁇ 95. When v ⁇ 30, it may be difficult to ensure a sufficient energy density of the battery. When v>95, operation at a high power may be difficult.
  • the positive electrode 201 may have a thickness of 10 ⁇ m or more and 500 ⁇ m or less. When the positive electrode 201 has a thickness of less than 10 ⁇ m, it may be difficult to ensure a sufficient energy density of the battery. When the positive electrode 201 has a thickness of more than 500 ⁇ m, operation at a high power may be difficult.
  • the electrolyte layer 202 is a layer including an electrolyte material.
  • the electrolyte material is, for example, a solid electrolyte material.
  • the electrolyte layer 202 may be a solid electrolyte layer.
  • the solid electrolyte layer may include, as a main component, the above-described solid electrolyte material according to Embodiment 1 or 2.
  • the solid electrolyte layer may include the above-described solid electrolyte material according to Embodiment 1 or 2, for example, in a weight percentage of 50% or more (50% by weight or more) relative to the whole solid electrolyte layer.
  • This feature provides further improved charge/discharge characteristics of the battery.
  • the solid electrolyte layer may include the above-described solid electrolyte material according to Embodiment 1 or 2, for example, in a weight percentage of 70% or more (70% by weight or more) relative to the whole solid electrolyte layer.
  • This feature provides further improved charge/discharge characteristics of the battery.
  • the solid electrolyte layer which may include, as a main component, the above-described solid electrolyte material according to Embodiment 1 or 2, may further include, for example, inevitable impurities or starting raw materials, by-products, and decomposition products during synthesis of the above-described solid electrolyte material.
  • the solid electrolyte layer may include the solid electrolyte material according to Embodiment 1 or 2, for example, in a weight percentage of 100% (100% by weight) relative to the whole solid electrolyte layer, except for impurities due to inevitable entry.
  • This feature provides further improved charge/discharge characteristics of the battery.
  • the solid electrolyte layer may be composed only of the solid electrolyte material according to Embodiment 1 or 2.
  • the solid electrolyte layer may be composed only of a solid electrolyte material different from the solid electrolyte material according to Embodiment 1 or 2.
  • the solid electrolyte material different from the solid electrolyte material according to Embodiment 1 or 2 include Li 2 MgX4, Li 2 FeX 4 , Li(Al, Ga, In)X 4 , Li 3 (Al, Ga, In)X 6 , and LiI (X: F, Cl, Br, I).
  • the solid electrolyte layer may simultaneously include the solid electrolyte material according to Embodiment 1 or 2, and the above-described solid electrolyte material different from the solid electrolyte material according to Embodiment 1 or 2. In this case, both materials may be uniformly diffused.
  • a layer composed of the solid electrolyte material according to Embodiment 1 or 2 and a layer composed of the above-described solid electrolyte material different from the solid electrolyte material according to Embodiment 1 or 2 may be sequentially disposed in the layer-stacking direction of the battery.
  • the solid electrolyte layer may have a thickness of 1 ⁇ m or more and 1000 ⁇ m or less. When the solid electrolyte layer has a thickness of less than 1 ⁇ m, the positive electrode 201 and the negative electrode 203 have a higher probability of short-circuit therebetween. When the solid electrolyte layer has a thickness of more than 1000 ⁇ m, operation at a high power may be difficult.
  • the negative electrode 203 includes a material having a property of storing and releasing metal ions (such as lithium ions).
  • the negative electrode 203 includes, for example, a negative electrode active material (such as negative electrode active material particles 205 ).
  • Examples of the negative electrode active material include metal materials, carbon materials, oxides, nitrides, tin compounds, and silicon compounds. Such a metal material may be a single metal. Alternatively, the metal material may be an alloy. Examples of the metal material include metallic lithium and lithium alloys. Examples of the carbon materials include natural graphite, coke, partially graphitized carbon, carbon fiber, spherical carbon, artificial graphite, and amorphous carbon. From the viewpoint of capacity density, silicon (Si), tin (Sn), silicon compounds, and tin compounds are preferably used. In the case of using a negative electrode active material having a low average reaction voltage, the solid electrolyte material according to Embodiment 1 or 2 exerts more strongly the effect of suppressing electrolysis.
  • the negative electrode active material particles 205 may have a median diameter of 0.1 ⁇ m or more and 100 ⁇ m or less. When the negative electrode active material particles 205 have a median diameter of less than 0.1 ⁇ m, in the negative electrode, the negative electrode active material particles 205 and the solid electrolyte particles 100 may not form a good diffusion state. This results in degradation of the charge/discharge characteristics of the battery. When the negative electrode active material particles 205 have a median diameter of more than 100 ⁇ m, lithium diffuses slowly in the negative electrode active material particles 205 . This may make it difficult for the battery to operate at a high power.
  • the negative electrode active material particles 205 may have a median diameter larger than the median diameter of the solid electrolyte particles 100 . In this case, a good diffusion state of the negative electrode active material particles 205 and the halide solid electrolyte material is formed.
  • the volume ratio “v:100 ⁇ v” of the negative electrode active material particles 205 and the solid electrolyte particles 100 included in the negative electrode 203 may satisfy 30 ⁇ v ⁇ 95.
  • v ⁇ 30 it may be difficult to ensure a sufficient energy density of the battery.
  • v>95 operation at a high power may be difficult.
  • the negative electrode 203 may have a thickness of 10 ⁇ m or more and 500 ⁇ m or less. When the negative electrode has a thickness of less than 10 ⁇ m, it may be difficult to ensure a sufficient energy density of the battery. When the negative electrode has a thickness of more than 500 ⁇ m, operation at a high power may be difficult.
  • At least one of the positive electrode 201 , the electrolyte layer 202 , and the negative electrode 203 may include, for the purpose of increasing the ion conductivity or improving the chemical stability and electrochemical stability, a sulfide solid electrolyte or an oxide solid electrolyte.
  • a sulfide solid electrolyte or an oxide solid electrolyte examples include Li 2 S—P 2 S 5 , Li 2 S—SiS 2 , Li 2 S—B 2 S 3 , Li 2 S—GeS 2 , Li 3.25 Ge 0.25 P 0.75 S 4 , and Li 10 GeP 2 S 12 .
  • oxide solid electrolyte examples include NASICON solid electrolytes represented by LiTi 2 (PO 4 ) 3 and element-substitution products thereof, (LaLi)TiO 3 -based perovskite solid electrolytes, LISICON solid electrolytes represented by Li 14 ZnGe 4 O 16 , Li 4 SiO 4 , LiGeO 4 , and element-substitution products thereof, garnet solid electrolytes represented by Li 7 La 3 Zr 2 O 12 and element-substitution products thereof, Li 3 N and H-substitution products thereof, and Li 3 PO 4 and N-substitution products thereof.
  • NASICON solid electrolytes represented by LiTi 2 (PO 4 ) 3 and element-substitution products thereof
  • (LaLi)TiO 3 -based perovskite solid electrolytes LISICON solid electrolytes represented by Li 14 ZnGe 4 O 16 , Li 4 SiO 4 , LiGeO 4 , and element-substitution products thereof
  • At least one of the positive electrode 201 , the electrolyte layer 202 , and the negative electrode 203 may include, for the purpose of increasing the ion conductivity, an organic polymer solid electrolyte.
  • the organic polymer solid electrolyte may be, for example, a compound of a polymer and a lithium salt.
  • the polymer may have an ethylene oxide structure. The presence of the ethylene oxide structure enables a high lithium salt content, which provides further increased ion conductivity.
  • lithium salt examples include LiPF 6 , LiBF 4 , LiSbF 6 , LiAsF 6 , LiSO 3 CF 3 , LiN(SO 2 CF 3 ) 2 , LiN(SO 2 C 2 F 5 ) 2 , LiN(SO 2 CF 3 )(SO 2 C 4 F 9 ), and LiC(SO 2 CF 3 ) 3 .
  • the lithium salt a single lithium salt selected from these may be used alone. Alternatively, as the lithium salt, a mixture of two or more lithium salts selected from these may be used.
  • At least one of the positive electrode 201 , the electrolyte layer 202 , and the negative electrode 203 may include, for the purpose of facilitating exchange of lithium ions and improving the power characteristics of the battery, a non-aqueous electrolyte solution, a gel electrolyte, or an ionic liquid.
  • the non-aqueous electrolyte solution includes a non-aqueous solvent and a lithium salt dissolved in the non-aqueous solvent.
  • the non-aqueous solvent include a cyclic carbonic acid ester solvent, a chain carbonic acid ester solvent, a cyclic ether solvent, a chain ether solvent, a cyclic ester solvent, a chain ester solvent, and a fluorocarbon solvent.
  • the cyclic carbonic acid ester solvent include ethylene carbonate, propylene carbonate, and butylene carbonate.
  • Examples of the chain carbonic acid ester solvent include dimethyl carbonate, ethyl methyl carbonate, and diethyl carbonate.
  • Examples of the cyclic ether solvent include tetrahydrofuran, 1,4-dioxane, and 1,3-dioxolane.
  • Examples of the chain ether solvent include 1,2-dimethoxyethane and 1,2-diethoxyethane.
  • Examples of the cyclic ester solvent include ⁇ -butyrolactone.
  • Examples of the chain ester solvent include methyl acetate.
  • Examples of the fluorocarbon solvent include fluoroethylene carbonate, methyl fluoropropionate, fluorobenzene, fluoroethyl methyl carbonate, and fluorodimethylene carbonate.
  • the non-aqueous solvent a single non-aqueous solvent selected from these may be used alone.
  • non-aqueous solvent two or more non-aqueous solvents selected from these may be used in combination.
  • the non-aqueous electrolyte solution may include at least one fluorocarbon solvent selected from the group consisting of fluoroethylene carbonate, methyl fluoropropionate, fluorobenzene, fluoroethyl methyl carbonate, and fluorodimethylene carbonate.
  • lithium salt examples include LiPF 6 , LiBF 4 , LiSbF 6 , LiAsF 6 , LiSO 3 CF 3 , LiN(SO 2 CF 3 ) 2 , LiN(SO 2 C 2 F 5 ) 2 , LiN(SO 2 CF 3 )(S 2 C 4 F 9 ), and LiC(SO 2 CF 3 ) 3 .
  • a single lithium salt selected from these may be used alone.
  • a mixture of two or more lithium salts selected from these may be used as the lithium salt.
  • the concentration of the lithium salt is, for example, in the range of 0.5 to 2 mol/l.
  • the gel electrolyte may be a polymer material prepared so as to contain a non-aqueous electrolyte solution.
  • the polymer material include polyethylene oxide, polyacrylonitrile, polyvinylidene fluoride, polymethyl methacrylate, and polymers having ethylene oxide bonds.
  • Examples of the cation constituting the ionic liquid include aliphatic chain quaternary salts such as tetraalkyl ammonium and tetraalkyl phosphonium; aliphatic cyclic ammoniums such as pyrrolidiniums, morpholiniums, imidazoliniums, tetrahydropyrimidiniums, piperaziniums, and piperidiniums; and nitrogen-containing heterocyclic aromatic cations such as pyridiniums and imidazoliums.
  • aliphatic chain quaternary salts such as tetraalkyl ammonium and tetraalkyl phosphonium
  • aliphatic cyclic ammoniums such as pyrrolidiniums, morpholiniums, imidazoliniums, tetrahydropyrimidiniums, piperaziniums, and piperidiniums
  • nitrogen-containing heterocyclic aromatic cations such as pyridiniums and
  • Examples of the anion constituting the ionic liquid include PF 6 ⁇ , BF 4 ⁇ , SbF 4 ⁇ , AsF 6 ⁇ , SO 3 CF 3 ⁇ , N(SO 2 CF 3 ) 2 ⁇ , N(SO 2 C 2 F 5 ) 2 ⁇ , N(SO 2 CF 3 )(SO 2 C 4 F 9 ) ⁇ , and C(SO 2 CF 3 ) 3 ⁇ .
  • the ionic liquid may contain lithium salt.
  • At least one of the positive electrode 201 , the electrolyte layer 202 , and the negative electrode 203 may include, for the purpose of improving adhesion between particles, a binder.
  • the binder is used in order to improve the binding property of the material constituting an electrode.
  • binder examples include polyvinylidene fluoride, polytetrafluoroethylene, polyethylene, polypropylene, aramid resin, polyamide, polyimide, polyamide-imide, polyacrylonitrile, polyacrylic acid, methyl polyacrylate ester, ethyl polyacrylate ester, hexyl polyacrylate ester, polymethacrylic acid, methyl polymethacrylate ester, ethyl polymethacrylate ester, hexyl polymethacrylate ester, polyvinyl acetate, polyvinylpyrrolidone, polyether, polyethersulfone, hexafluoropolypropylene, styrene-butadiene rubber, and carboxymethylcellulose.
  • the binder may be a copolymer of two or more materials selected from tetrafluoroethylene, hexafluoroethylene, hexafluoropropylene, perfluoroalkyl vinyl ether, vinylidene fluoride, chlorotrifluoroethylene, ethylene, propylene, pentafluoropropylene, fluoromethyl vinyl ether, acrylic acid, and hexadiene. Alternatively, two or more selected from these may be mixed and used as the binder.
  • At least one of the positive electrode 201 and the negative electrode 203 may include a conductive agent as needed.
  • the conductive agent is used in order to reduce the electrode resistance.
  • the conductive agent include graphites such as natural graphite and artificial graphite; carbon blacks such as acetylene black and Ketjen black; conductive fibers such as carbon fiber and metal fiber; carbon fluoride; powders of metals such as aluminum; conductive whiskers such as zinc oxide and potassium titanate; conductive metal oxides such as titanium oxide; and conductive polymers such as polyaniline, polypyrrole, and polythiophene.
  • Use of, as the conductive agent, such a carbon conductive agent achieves a reduction in the costs.
  • the battery according to Embodiment 2 may be provided as batteries having various shapes such as a coin shape, a cylindrical shape, a prismatic shape, a sheet shape, a button shape, a flat shape, and a stacked layer shape.
  • FIG. 2 is a schematic view illustrating a method of evaluating lithium-ion conductivity.
  • a pressing die 300 is constituted by a die 301 , which is electronically insulating and composed of polycarbonate, and an upper punch 303 and a lower punch 302 , which are electron conductive and composed of stainless steel.
  • the structure illustrated in FIG. 2 was used to evaluate ion conductivity by the following method.
  • Example A1 In a dry atmosphere at a dew point of ⁇ 30° C. or less, the powder of the solid electrolyte material of Example A1 was charged into the pressing die 300 , and uniaxially pressed at 400 MPa, to prepare a conductivity measurement cell of Example A1.
  • the Cole-Cole plot based on the measurement results of impedance is illustrated in FIG. 3 .
  • ⁇ represents ion conductivity
  • S represents the area of the electrolyte (in FIG. 2 , the inner diameter of the die 301 );
  • R SE represents the resistance of the solid electrolyte determined by the above-described impedance measurement; and
  • t represents the thickness of the electrolyte (in FIG. 2 , the thickness of the compact of the plurality of solid electrolyte particles 100 ).
  • the solid electrolyte material of Example A1 was found to have an ion conductivity at 22° C. of 1.2 ⁇ 10 ⁇ 3 S/cm.
  • FIG. 4 A is a graph illustrating XRD patterns.
  • an X-ray diffractometer (MiniFlex 600 from Rigaku Corporation) was used to measure the X-ray diffraction pattern in a dry environment at a dew point of ⁇ 45° C. or less.
  • the X-ray source Cu-K ⁇ radiation was used.
  • a ave was calculated by Formula (2) and found to be 5.232 ⁇ .
  • Example A1 and LiCoO 2 serving as an active material were weighed in a volume ratio of 70:30. These were mixed in an agate mortar, to prepare a mixture.
  • the solid electrolyte material of Example A1 in an amount corresponding to a thickness of 700 ⁇ m, 8.5 mg of the above-described mixture, and 16.5 mg of A1 powder were stacked in this order. This stack was pressed at a pressure of 300 MPa, to obtain a first electrode and a solid electrolyte layer.
  • metal In thickness: 200 ⁇ m
  • This stack was pressed at a pressure of 80 MPa, to prepare a stack constituted by the first electrode, the solid electrolyte layer, and a second electrode.
  • the stack was made to be overlain by and underlain by stainless steel current collectors, and current collection leads were attached to the current collectors.
  • the charge/discharge test of the secondary battery of Example A1 was performed in the following manner.
  • the battery was subjected to constant current charging at a current corresponding to 0.05 C rate (20 hour rate) relative to the theoretical capacity of the battery.
  • the charging was terminated at a voltage of 3.6 V.
  • the initial discharge capacity of the secondary battery of Example A1 was found to be 0.467 mAh.
  • Examples A2 to A11 within a glove box having a dry and low-oxygen-content atmosphere maintained at a dew point of ⁇ 60° C. or less and an oxygen content of 5 ppm or less, raw material powders were weighed so as to have predetermined compositions.
  • the compositions of solid electrolytes produced in Examples A2 to A11 are described later in Table 1.
  • a planetary ball mill was used to perform milling processing for 12 hours at 600 rpm.
  • heat treatment was respectively performed at 500° C. and 300° C. for 5 hours.
  • Example A1 In a glove box having a dry and low-oxygen-content atmosphere maintained at a dew point of ⁇ 90° C. or less and an oxygen content of 5 ppm or less, the same method as in Example A1 above was performed to prepare conductivity measurement cells of Examples A2 to A11.
  • Example A1 the same method as in Example A1 above was performed to measure ion conductivity.
  • Example A1 The same method as in Example A1 above was performed to measure the crystal structure of each of the solid electrolyte materials of Examples A2 to A11.
  • the resultant diffraction pattern in which the abscissa axis represents values of q/q 2 is illustrated in FIG. 4 B .
  • each of the solid electrolyte materials of Examples A2 to A11 and LiCoO 2 serving as a positive electrode active material were weighed in a volume ratio of 30:70. These were mixed in an agate mortar. Thus, positive electrode mixtures of Examples A2 to A11 were prepared.
  • Example A1 Except for these, the same method as in Example A1 above was performed to produce secondary batteries of Examples A2 to A11.
  • Example A2 The same method as in Example A1 above was performed to subject the secondary batteries of Examples A2 to A11 to the charge/discharge test.
  • the initial discharge characteristics of Examples A2 to A11 were similar to those of Example A1, and good charge/discharge characteristics were obtained.
  • the initial discharge characteristics in Example A2 are illustrated in FIG. 5 .
  • the discharge capacity of Example A2 was found to be 0.657 mAh.
  • Examples B1 to B13 within a glove box having a dry and low-oxygen-content atmosphere maintained at a dew point of ⁇ 60° C. or less and an oxygen content of 5 ppm or less, raw material powders were weighed.
  • the compositions of solid electrolytes produced in Examples B1 to B13 are described later in Table 2.
  • Example A1 The same method as in Example A1 above was performed to measure the crystal structure of each of the solid electrolyte materials of Examples B1 to B13.
  • Example A1 In a glove box having a dry and low-oxygen-content atmosphere maintained at a dew point of ⁇ 90° C. or less and an oxygen content of 5 ppm or less, the same method as in Example A1 above was performed to prepare conductivity measurement cells of Examples B1 to B13.
  • Example A1 the same method as in Example A1 above was performed to measure ion conductivity.
  • each of the solid electrolyte materials of Examples B1 to B13 and LiCoO 2 serving as a positive electrode active material were weighed in a volume ratio of 30:70. These were mixed in an agate mortar. Thus, positive electrode mixtures of Examples B1 to B13 were prepared.
  • Example A1 Except for these, the same method as in Example A1 above was performed to produce secondary batteries of Examples B1 to B13.
  • Example A1 The same method as in Example A1 above was performed to subject the secondary batteries of Examples B1 to B13 to the charge/discharge test.
  • the initial discharge characteristics of Examples B1 to B13 were similar to those of Example A1, and good charge/discharge characteristics were obtained.
  • Comparative Examples 1 to 3 within a glove box having a dry and low-oxygen-content atmosphere maintained at a dew point of ⁇ 60° C. or less and an oxygen content of 5 ppm or less, raw material powders were weighed. The compositions of solid electrolytes produced in Comparative Examples 1 to 3 are described later in Table 3. In Comparative Example 3, subsequently, heat treatment was performed at 200° C. for 1 hour.
  • Example A1 Except for these, the same method as in Example A1 above was performed to produce solid electrolyte materials of Comparative Examples 1 to 3.
  • Example A1 The same method as in Example A1 above was performed to measure the crystal structure of each of the solid electrolyte materials of Comparative Examples 1 to 3.
  • the resultant diffraction pattern in which the abscissa axis represents values of q/q 1 ′ is illustrated in FIG. 78 .
  • Example A1 In a glove box having a dry and low-oxygen-content atmosphere maintained at a dew point of ⁇ 90° C. or less and an oxygen content of 5 ppm or less, the same method as in Example A1 above was performed to prepare conductivity measurement cells of Comparative Examples 1 to 3.
  • Example A1 the same method as in Example A1 above was performed to measure ion conductivity.
  • the solid electrolyte material of Comparative Example 2 was weighed in a volume ratio of 30:70. These were mixed in an agate mortar. Thus, the positive electrode mixture of Comparative Example 2 was prepared.
  • Example A1 The same method as in Example A1 above was performed to subject the secondary battery of Comparative Example 2 to the charge/discharge test. Regarding initial discharge characteristics of Comparative Example 2, the battery substantially did not discharge and did not operate.
  • Examples A1 to A11 and B1 to B13 have been found to exhibit high ion conductivities of 1 ⁇ 10 ⁇ 4 S/cm or more at or about room temperature, compared with Comparative Examples 1 to 3.
  • Examples A1 to A11 peaks were observed in ranges of q/q 2 of 0.50 to 0.52, 1.28 to 1.30, and 1.51 to 1.54, which are characteristic peaks observed when sublattices composed of halogen ions have a hexagonal closest packed structure or a distorted hexagonal closest packed structure.
  • Examples B1 to B13 peaks were observed in ranges of q/q′ of 1.14-1.17, 1.625-1.645, 1.88-1.94, and 1.90-2.10, which are characteristic peaks observed when sublattices composed of halogen ions have a cubic closest packed structure or a distorted cubic closest packed structure.
  • Example A1 comparison between Example A1 and Comparative Example 3 has revealed the following: in spite of the same constituent elements, the structure of Example A1 provided to have an a ave /a LiX of more than 1.018 exhibits markedly increased ion conductivity, compared with Comparative Example 3.
  • Example 1 the battery exhibited charge/discharge operations at room temperature.
  • Comparative Example 2 discharge capacity was not substantially detected, and operations of the battery were not confirmed.
  • the materials for Examples A1 to A11 and B1 to B13 do not include sulfur as a constituent element, so that generation of hydrogen sulfide does not occur.
  • the solid electrolyte material according to the present disclosure is an electrolyte material that does not generate hydrogen sulfide, exhibits a high lithium-ion conductivity, and exhibits good charge/discharge operations.

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CN111279432A (zh) 2020-06-12
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